CN108132174A - The sample pretreating method of sodium sulfocyanate in a kind of detection liquid food - Google Patents
The sample pretreating method of sodium sulfocyanate in a kind of detection liquid food Download PDFInfo
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- CN108132174A CN108132174A CN201711240081.2A CN201711240081A CN108132174A CN 108132174 A CN108132174 A CN 108132174A CN 201711240081 A CN201711240081 A CN 201711240081A CN 108132174 A CN108132174 A CN 108132174A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention discloses a kind of sample pretreating methods for detecting sodium sulfocyanate in liquid food, are related to technical field of food detection, include the following steps：Liquid food sample is taken to be placed in triangular flask, adds solution of trichloroacetic acid, stands after mixing, filters, obtains supernatant A, for use；Ultra-pure water dissolved dilution is added in into supernatant A, is transferred in volumetric flask, ultrasonic vibration, precipitating reagent, whirlpool precipitation, with ultra-pure water constant volume, centrifugal treating, Aspirate supernatant B and with filtering with microporous membrane to get sample solution are separately added into volumetric flask.The present invention can effectively remove the impurity such as protein, fat, the grease in detection liquid food, and pretreatment is simple, favorable reproducibility, shorten sample processing time, impurity is few after processing, and the accuracy and precision of detection are high, disclosure satisfy that the quick testing requirements of a large amount of samples.
Description
Technical field
The present invention relates to technical field of food detection more particularly to a kind of sample for detecting sodium sulfocyanate in liquid food are pre-
Processing method.
Background technology
Food security be common people concern hot spot and tender subject, the personal safety as well as the property safety concerning the people.In recent years
Come, food-safety problem takes place frequently, sodium sulfocyanate, melamine, tonyred, carcinogenic malicious rice, Fuyang doll with big head milk powder, platform modeling agent
And tens of food safety affairs such as clenbuterol hydrochloride are investigated and prosecuted after exposing, and are aroused great concern.At present, food security
Problem mainly includes the following aspects：Chemical hazard, biotoxin, microbes harm, food adulteration, biological transgenosis
Food and bioterrorism event etc..Various food security standards and a series of have also been launched respectively for these aspect China
Food security universaling analysis method.The project of detection mainly includes antibiotic residual quantity, content of beary metal and food additives
Amount etc., the method for use is generally chemical analysis, is given birth to including chromatography, mass spectral analysis and spectrum analysis and modern molecular
Object technology etc..But it is required to just be detected after pre-processing food.
Sodium sulfocyanate has certain bacteriostasis, but belongs to the poisonous and hazardous non-edible additives matter to human body, due to
The content of filling material is less in liquid food, and complicated component, can influence testing result, thus sample pretreatment typical time compared with
Long, step is more, causes sample pretreatment error larger, it is therefore desirable to provide sodium sulfocyanate in a kind of new detection liquid food
Sample pretreating method.
Invention content
Technical problems based on background technology, the present invention propose a kind of sample for detecting sodium sulfocyanate in liquid food
Product preprocess method, after preprocess method processing, testing result is accurate, and error is small.
A kind of sample pretreating method for detecting sodium sulfocyanate in liquid food proposed by the present invention, includes the following steps：
S1, liquid food sample is taken to be placed in triangular flask, adds in solution of trichloroacetic acid, stand after mixing, filtered, obtain
Supernatant A, for use；
S2, ultra-pure water dissolved dilution is added in into supernatant A, be transferred in volumetric flask, ultrasonic vibration, divided into volumetric flask
Do not add in precipitating reagent, whirlpool precipitation with ultra-pure water constant volume, centrifugal treating, Aspirate supernatant B and with filtering with microporous membrane, obtains
Sample solution, you can.
Preferably, include the following steps：
S1,10-15mL liquid food samples is taken to be placed in triangular flask, adds in 2-5mL solution of trichloroacetic acid, side edged stirs
It mixes, stands 15-25min after mixing, with quantitative filter paper filtering in totally dry triangular flask, it is for use to obtain supernatant A；
S2,20-30ml ultra-pure water dissolved dilutions are added in into supernatant A, divides 3-5 times and be transferred to supernatant A dilution
In 50mL volumetric flasks, taken out after ultrasonic vibration extraction, be separately added into precipitating reagent into volumetric flask, whirlpool precipitation 1-2min, with super
Pure water constant volume is simultaneously uniformly mixed, and is placed in centrifuge tube and is carried out centrifugal treating, Aspirate supernatant B and with filtering with microporous membrane, is obtained
Sample solution, you can.
Preferably, the precipitating reagent is by 0.5-1.5mL potassium ferrocyanides, 0.5-1.5mL zinc acetates, 0.5-1.5mL sulfuric acid
Ammonium mixes.
Preferably, the aperture of the miillpore filter is 1-10 μm.
Preferably, the process conditions of the centrifugal treating are：Centrifugation time 10-15min, centrifugal rotational speed 3000-3500r/
min。
Preferably, the power of the ultrasonic vibration is 40-50W, ultrasonic 8-15min
Advantageous effect：Trichloroacetic acid is added in the present invention in sample, protein precipitation can be removed, supernatant is taken to add in
Ultrapure water dissolution extraction, adds precipitating reagent, and it is miscellaneous can effectively to remove protein, fat, the grease detected in liquid food etc.
Matter is extracted using ultra-pure water, and subsequent detection will not be impacted, and is detected again after finally taking supernatant liquid filtering, and pretreatment is simple,
Favorable reproducibility shortens sample processing time, and impurity is few after processing, and the accuracy and precision of detection are high, disclosure satisfy that a large amount of
The quick testing requirements of sample.
Specific embodiment
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of sample pretreating method for detecting sodium sulfocyanate in liquid food proposed by the present invention, includes the following steps：
S1,10mL liquid food samples is taken to be placed in triangular flask, adds 2mL solution of trichloroacetic acid, stirring while adding, mixing is equal
15min is stood after even, with quantitative filter paper filtering in totally dry triangular flask, it is for use to obtain supernatant A；
S2, the ultrapure water dissolutions of 20ml are added in into supernatant A, divides 3 times and supernatant A dilution is transferred to 50mL volumetric flasks
In, taken out after ultrasonic vibration extraction 8min, ultrasonic power 40W is separately added into precipitating reagent into volumetric flask, precipitating reagent by
0.5mL potassium ferrocyanides, 0.5mL zinc acetates, 0.5mL ammonium sulfate mix, and whirlpool precipitation 1min with ultra-pure water constant volume and is mixed
It closes uniformly, is placed in centrifuge tube and carries out centrifugal treating, centrifugation time 10min, centrifugal speed 3000r/min, Aspirate supernatant B is simultaneously
With filtering with microporous membrane, sample solution is obtained, you can.
Embodiment 2：
A kind of sample pretreating method for detecting sodium sulfocyanate in liquid food proposed by the present invention, includes the following steps：
S1,15mL liquid food samples is taken to be placed in triangular flask, adds 5mL solution of trichloroacetic acid, stirring while adding, mixing is equal
25min is stood after even, with quantitative filter paper filtering in totally dry triangular flask, it is for use to obtain supernatant A；
S2, the ultrapure water dissolutions of 30ml are added in into supernatant A, divides 5 times and supernatant A dilution is transferred to 50mL volumetric flasks
In, taken out after ultrasonic vibration extraction 15min, ultrasonic power 50W is separately added into precipitating reagent into volumetric flask, precipitating reagent by
1.5mL potassium ferrocyanides, 1.5mL zinc acetates, 1.5mL ammonium sulfate mix, and whirlpool precipitation 2min with ultra-pure water constant volume and is mixed
It closes uniformly, is placed in centrifuge tube and carries out centrifugal treating, centrifugation time 15min, centrifugal speed 3500r/min, Aspirate supernatant B is simultaneously
With filtering with microporous membrane, sample solution is obtained, you can.
Embodiment 3：
A kind of sample pretreating method for detecting sodium sulfocyanate in liquid food proposed by the present invention, includes the following steps：
S1,12mL liquid food samples is taken to be placed in triangular flask, adds 3mL solution of trichloroacetic acid, stirring while adding, mixing is equal
20min is stood after even, with quantitative filter paper filtering in totally dry triangular flask, it is for use to obtain supernatant A；
S2, the ultrapure water dissolutions of 25ml are added in into supernatant A, divides 4 times and supernatant A dilution is transferred to 50mL volumetric flasks
In, it is taken out after ultrasonic vibration extraction 11min, ultrasonic power 45W is separately added into precipitating reagent into volumetric flask, and precipitating reagent is by 1mL
Potassium ferrocyanide, 1mL zinc acetates, 1mL ammonium sulfate mix, and whirlpool precipitation 2min with ultra-pure water constant volume and is uniformly mixed, puts
Centrifugal treating, centrifugation time 13min, centrifugal speed 3200r/min are carried out in centrifuge tube, Aspirate supernatant B is simultaneously filtered with micropore
Membrane filtration obtains sample solution, you can.
Embodiment 4：
A kind of sample pretreating method for detecting sodium sulfocyanate in liquid food proposed by the present invention, includes the following steps：
S1,11mL liquid food samples is taken to be placed in triangular flask, adds 3mL solution of trichloroacetic acid, stirring while adding, mixing is equal
18min is stood after even, with quantitative filter paper filtering in totally dry triangular flask, it is for use to obtain supernatant A；
S2, the ultrapure water dissolutions of 23ml are added in into supernatant A, divides 4 times and supernatant A dilution is transferred to 50mL volumetric flasks
In, taken out after ultrasonic vibration extraction 13min, ultrasonic power 42W is separately added into precipitating reagent into volumetric flask, precipitating reagent by
0.8mL potassium ferrocyanides, 0.8mL zinc acetates, 0.8mL ammonium sulfate mix, whirlpool precipitation 1.5min, with ultra-pure water constant volume simultaneously
It is uniformly mixed, is placed in centrifuge tube and carries out centrifugal treating, centrifugation time 14min, centrifugal speed 3100r/min, Aspirate supernatant B
And with filtering with microporous membrane, sample solution is obtained, you can.
Embodiment 5：
A kind of sample pretreating method for detecting sodium sulfocyanate in liquid food proposed by the present invention, includes the following steps：
S1,14mL liquid food samples is taken to be placed in triangular flask, adds 4mL solution of trichloroacetic acid, stirring while adding, mixing is equal
22min is stood after even, with quantitative filter paper filtering in totally dry triangular flask, it is for use to obtain supernatant A；
S2, the ultrapure water dissolutions of 28ml are added in into supernatant A, divides 5 times and supernatant A dilution is transferred to 50mL volumetric flasks
In, taken out after ultrasonic vibration extraction 10min, ultrasonic power 48W is separately added into precipitating reagent into volumetric flask, precipitating reagent by
1.3mL potassium ferrocyanides, 1.3mL zinc acetates, 1.3mL ammonium sulfate mix, and whirlpool precipitation 2min with ultra-pure water constant volume and is mixed
It closes uniformly, is placed in centrifuge tube and carries out centrifugal treating, centrifugation time 12min, centrifugal speed 3400r/min, Aspirate supernatant B is simultaneously
With filtering with microporous membrane, sample solution is obtained, you can.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of sample pretreating method for detecting sodium sulfocyanate in liquid food, which is characterized in that include the following steps：
S1, liquid food sample is taken to be placed in triangular flask, adds in solution of trichloroacetic acid, stand after mixing, filtered, obtain supernatant
Liquid A, for use；
S2, ultra-pure water dissolved dilution is added in into supernatant A, be transferred in volumetric flask, ultrasonic vibration, added respectively into volumetric flask
Enter precipitating reagent, whirlpool precipitation with ultra-pure water constant volume, centrifugal treating, Aspirate supernatant B and with filtering with microporous membrane, obtains sample
Solution, you can.
2. the sample pretreating method of sodium sulfocyanate in liquid food is detected according to claim 1, which is characterized in that including
Following steps：
S1,10-15mL liquid food samples is taken to be placed in triangular flask, adds in 2-5mL solution of trichloroacetic acid, it is stirring while adding, it mixes
15-25min is stood after closing uniformly, with quantitative filter paper filtering in totally dry triangular flask, it is for use to obtain supernatant A；
S2,20-30ml ultra-pure water dissolved dilutions are added in into supernatant A, divides 3-5 times and supernatant A dilution is transferred to 50mL
It in volumetric flask, is taken out after ultrasonic vibration extraction, precipitating reagent is separately added into volumetric flask, whirlpool precipitation 1-2min uses ultra-pure water
Constant volume is simultaneously uniformly mixed, and is placed in centrifuge tube and is carried out centrifugal treating, Aspirate supernatant B and with filtering with microporous membrane, obtains sample
Solution, you can.
3. the sample pretreating method of sodium sulfocyanate in detection liquid food according to claim 1 or claim 2, which is characterized in that
The precipitating reagent is mixed by 0.5-1.5mL potassium ferrocyanides, 0.5-1.5mL zinc acetates, 0.5-1.5mL ammonium sulfate.
4. the sample pretreating method of sodium sulfocyanate in detection liquid food according to claim 1 or claim 2, which is characterized in that
The aperture of the miillpore filter is 1-10 μm.
5. the sample pretreating method of sodium sulfocyanate in detection liquid food according to claim 1 or claim 2, which is characterized in that
The process conditions of the centrifugal treating are：Centrifugation time 10-15min, centrifugal rotational speed 3000-3500r/min.
6. the sample pretreating method of sodium sulfocyanate in detection liquid food according to claim 1 or claim 2, which is characterized in that
The power of the ultrasonic vibration is 40-50W, ultrasonic 8-15min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711240081.2A CN108132174A (en) | 2017-11-30 | 2017-11-30 | The sample pretreating method of sodium sulfocyanate in a kind of detection liquid food |
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| CN201711240081.2A CN108132174A (en) | 2017-11-30 | 2017-11-30 | The sample pretreating method of sodium sulfocyanate in a kind of detection liquid food |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112730371A (en) * | 2020-11-26 | 2021-04-30 | 中国科学院合肥物质科学研究院 | Sample pretreatment method for detecting cyanide by using surface-enhanced Raman scattering composite substrate |
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| US20040265800A1 (en) * | 2003-06-30 | 2004-12-30 | Sysmex Corporation | Sample pretreatment solution for immunological test and method for using the same |
| CN201382930Y (en) * | 2009-02-27 | 2010-01-13 | 陕西出入境检验检疫局检验检疫技术中心 | Rapid testing kit for sodium sulfocyanate in liquid milk |
| CN102608109A (en) * | 2012-03-03 | 2012-07-25 | 河北省科学院生物研究所 | Thiocyanate radical detecting kit and application thereof |
| CN103439312B (en) * | 2013-09-06 | 2016-03-30 | 哈尔滨工业大学 | A kind of method of based on Surface enhanced raman spectroscopy technology, the content of sodium thiocyanate in milk being carried out to detect fast |
| CN107328885A (en) * | 2017-08-25 | 2017-11-07 | 天津量信检验认证技术有限公司 | The pretreatment of solid-state food acesulfame potassium and quick determination method |
-
2017
- 2017-11-30 CN CN201711240081.2A patent/CN108132174A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040265800A1 (en) * | 2003-06-30 | 2004-12-30 | Sysmex Corporation | Sample pretreatment solution for immunological test and method for using the same |
| CN201382930Y (en) * | 2009-02-27 | 2010-01-13 | 陕西出入境检验检疫局检验检疫技术中心 | Rapid testing kit for sodium sulfocyanate in liquid milk |
| CN102608109A (en) * | 2012-03-03 | 2012-07-25 | 河北省科学院生物研究所 | Thiocyanate radical detecting kit and application thereof |
| CN103439312B (en) * | 2013-09-06 | 2016-03-30 | 哈尔滨工业大学 | A kind of method of based on Surface enhanced raman spectroscopy technology, the content of sodium thiocyanate in milk being carried out to detect fast |
| CN107328885A (en) * | 2017-08-25 | 2017-11-07 | 天津量信检验认证技术有限公司 | The pretreatment of solid-state food acesulfame potassium and quick determination method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112730371A (en) * | 2020-11-26 | 2021-04-30 | 中国科学院合肥物质科学研究院 | Sample pretreatment method for detecting cyanide by using surface-enhanced Raman scattering composite substrate |
| CN112730371B (en) * | 2020-11-26 | 2023-10-03 | 中国科学院合肥物质科学研究院 | Sample pretreatment method for detecting cyanide by surface enhanced Raman scattering composite substrate |
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Application publication date: 20180608 |